CN107746985A - A kind of preparation method of stratiform interworking architecture composite - Google Patents
A kind of preparation method of stratiform interworking architecture composite Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/0605—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances by sublimating
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
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- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
- C22C1/1021—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform the preform being ceramic
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1073—Infiltration or casting under mechanical pressure, e.g. squeeze casting
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
Abstract
The present invention relates to a kind of preparation method of stratiform interworking architecture composite, belong to technical field of composite materials.The present invention is by sodium carboxymethylcellulose,Glucose is added in deionized water,Stirring,Plus silicon carbide again,Aluminum oxide,It is transferred to after zirconium oxide stirring in ball mill,Ball milling,Obtain ceramic slurry,Take Teflon mould,Ceramic slurry is sprayed into mould again,After sprayed,Stand directional solidification,Obtain solidifying body,It is placed in after solidifying body is stripped in vacuum freezing drying oven,It is freeze-dried to obtain layered porous ceramic body,Layered porous ceramic body is placed in tube furnace,Heated under air atmosphere,After insulation reaction again under argon atmosphere,Heating,Insulation reaction is cooled to room temperature,Obtain layered porous ceramics,Layered porous ceramics are placed in high-pressure impregnation stove,And the placing aluminium alloy at the top of ceramics,Reheat,Enable aluminum alloy to melt,And it is passed through argon gas,Room temperature is naturally cooled to after insulation again,Obtain stratiform interworking architecture composite.
Description
Technical field
The present invention relates to a kind of preparation method of stratiform interworking architecture composite, belong to technical field of composite materials.
Background technology
With the fast development in the fields such as building, traffic, space flight and aviation and electronics industry, the application performance of material is carried
Higher requirement is gone out.Traditional homogenous material（Such as ceramics, metal and high polymer material）It can not meet that commercial Application will already
Ask.Following significant challenge is new stronger, more tough and lightweight the structural material of exploitation.Metal-base composites is wherein
One of optimal material, it have concurrently metal and it is ceramic the advantages of, not only with high specific strength, high ratio modulus, wear-resistant, weight
Gently, higher operating temperature can be born, but also there is good thermophysical property, thus both can be used as it is against corrosion, wear-resisting,
Resistant to elevated temperatures structural member, it is growing but also as conduction, heat conduction, radiation-resistant functional material, its demand.But sorry
It is that this kind of material also seldom realizes commercialization at present, traces it to its cause：First, production cost is high, secondary operation is difficult；Second, with
The increase of ceramic phase reinforcement content, the toughness of composite decline, and work to break is reduced, and performance is unstable, uses inadequate peace
Entirely, this is also that ceramic particle reinforced metal base composites never have the bottleneck problem solved for many years.Want to reach material
Optimum performance, it is necessary to the internal relation between material structure parameter and mechanical property and interaction are fully understood, in addition, having
The coming of new technology of synthesizing block structural material is sought and developed to necessity.The multicomponent of material, multi-functional and structure function one
Bodyization has turned into the inexorable trend of material science development.Mutually strengthen brittlement phase using ductility to improve fracture toughness, this thought
It is long-standing in the design of composite, significant effect is also achieved in practice.However, intensity and toughness are mutually exclusive
Two kinds of performances.The mechanics performance for reaching optimal is often the result that both performances meet each other half way.In metal-based compound material
In material, people extensively study the factor for influenceing mechanical response at present, including matrix composition, enhancing phase species and shape
Interfacial structure and combination between state, volume fraction, distribution situation and enhancing phase and matrix etc..Meanwhile mechanics study confirms,
Enhancing phase containing same volume but different-shape in the composite（Such as stratiform, graininess, threadiness）When, layer structure will be in
Existing maximum toughening effect, next to that threadiness and graininess.It is and final high tough（That is high damage tolerance）Composite obtains
Effective control to microstructure in component material performance and multi-scale range must be relied primarily on.In optimization composite obdurability
During, the biomaterial in the Nature gives people and much enlightened.Biomaterial (such as dentine, bone, shell) passes through
The evolution of hundreds of millions of years, form the fine structure adaptable with environment and functional requirement, show Traditional Man synthetic material without
The excellent properties of method analogy.Shell pearl layer is the outstanding representative in numerous biomaterials, and it is by hard phase and the soft arrangement that alternates
Nanoscale " brick-mud " composite construction is formd, therefore not only there is higher intensity, but also shows surprising fracture toughness
And good wearability, turn into and prepared lightweight, the model structure of high-strength tenacity bionic laminar composite.Nearest
20 years, the great interest of academia is caused using the composite of bionic principle preparation class pearl shell structure.It is but traditional
Technology（As flow casting molding, hot pressed sintering, reaction-sintered, vapour deposition infiltration etc.）It is difficult to imitated as the block of shell fine structure
Composite, the mechanical property of material can not be made to reach optimal.
The content of the invention
The technical problems to be solved by the invention：For current ceramic-metal composite poor mechanical property, anti-wear performance
A kind of the problem of poor, there is provided preparation method of stratiform interworking architecture composite.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of preparation method of stratiform interworking architecture composite, it is characterised in that specifically preparation process is：
（1）Row is transferred to after taking sodium carboxymethylcellulose, glucose, deionized water, carborundum, aluminum oxide, zirconium oxide well mixed
8 ~ 10h of ball milling, obtains ceramic slurry in planetary high energy ball mill；
（2）Ceramic slurry is sprayed into Teflon mould, 2 ~ 3h of directional solidification is stood, obtains solidifying body；
（3）40 ~ 48h of freeze-drying in vacuum freezing drying oven is placed in after solidifying body is stripped, obtains layered porous ceramic body；
（4）Layered porous ceramic body is placed in tube furnace and sintered, is cooled to room temperature, obtains layered porous ceramics；
（5）Layered porous ceramics are placed in high-pressure impregnation stove, and the placing aluminium alloy at the top of ceramics, vacuumize and be heated to
800 ~ 900 DEG C are enabled aluminum alloy to melt, and 450 ~ 500 DEG C of 10 ~ 12h of insulation are cooled to after being passed through 10 ~ 15min of argon pressurization, then natural
Room temperature is cooled to, obtains stratiform interworking architecture composite.
Step（1）The parts by weight of each component raw material are：8 ~ 10 parts of sodium carboxymethylcelluloses, 8 ~ 10 parts of glucose, 700
~ 750 parts of deionized waters, 200 ~ 240 parts of carborundum, 50 ~ 60 parts of aluminum oxide, 8 ~ 10 parts of zirconium oxides.
Step（2）The directional solidification is that to control Teflon mould bottom temp be -30 ~ -20 DEG C, then by ceramic slurry
Material is sprayed into mould with 10 ~ 20mL/min.
Step（3）Pressure is 1 ~ 10Pa in the vacuum freezing drying oven, and temperature is -60 ~ -50 DEG C.
Step（4）The sintering process is is warming up to 1100 ~ 1200 DEG C under air atmosphere with 5 DEG C/min, insulation reaction
60 ~ 80min, then 1500 ~ 1600 DEG C are warming up under argon atmosphere, 2 ~ 3h of insulation reaction, the heating, cooling speed is 5 DEG C/
min。
Step（5）The high-pressure impregnation furnace pressure is 1 ~ 10Pa, and the moulding pressure is 2 ~ 3MPa.
Compared with other method, advantageous effects are the present invention：
The present invention makes slurry uniformly sprawl simultaneously directional solidification, fixed by the way that slurry is sprayed into the mould with thermograde
Into process of setting, ice crystal in ceramic slurry oriented growth, the ice crystal forward position that ceramic particle is constantly grown since cold end
" exclusion " to ice crystal grain boundaries, a large amount of ceramic particles are arranged along crystal boundary, ultimately form the friendship of ice crystal layer and ceramic particle accumulation horizon
For arrangement, then solidifying body is positioned in low-temp low-pressure environment, deionized water ice crystal is distilled, then enter to the base substrate of freeze-drying
After row sintering processes, layered porous ceramics can be obtained, then are penetrated into aluminium alloy in layer structure with pressure infiltration method, form tool
There are lightweight, high-modulus, high-strength tenacity, wear-resisting stratiform interworking architecture composite.
Embodiment
8 ~ 10g sodium carboxymethylcelluloses are taken, 8 ~ 10g glucose is added in 700 ~ 750mL deionized waters, with 300 ~ 400r/
Min stirs 20 ~ 30min, adds 200 ~ 240g carborundum, 50 ~ 60g aluminum oxide, 8 ~ 10g zirconium oxides, continue stirring 20 ~
It is transferred to after 30min in planetary high-energy ball mill, with 100 ~ 150r/min, 8 ~ 10h of ball milling, obtains ceramic slurry, take polytetrafluoroethylene (PTFE)
Mould, and it is -30 ~ -20 DEG C to control bottom temp, then ceramic slurry is sprayed into mould with 10 ~ 20mL/min, it is sprayed
Afterwards, 2 ~ 3h of directional solidification is stood, solidifying body is obtained, is placed in after solidifying body is stripped in vacuum freezing drying oven, in 1 ~ 10Pa, -60
40 ~ 48h is freeze-dried at ~ -50 DEG C, layered porous ceramic body is obtained, layered porous ceramic body is placed in tube furnace, in sky
Atmosphere with 5 DEG C/min is heated to 1100 ~ 1200 DEG C under enclosing, and is heated to again under argon atmosphere after 60 ~ 80min of insulation reaction
1500 ~ 1600 DEG C, room temperature is cooled to 5 DEG C/min after 2 ~ 3h of insulation reaction, layered porous ceramics is obtained, layered porous ceramics is put
In in high-pressure impregnation stove, and the placing aluminium alloy at the top of ceramics, it is 1 ~ 10Pa to be evacuated to furnace pressure, then is added with 5 DEG C/min
Heat enables aluminum alloy to melt, and it be 2 ~ 3MPa to be passed through argon gas to furnace pressure to 800 ~ 900 DEG C, after 10 ~ 15min of insulation with 5 DEG C/
Min is cooled to 450 ~ 500 DEG C, is incubated 10 ~ 12h, then naturally cools to room temperature, obtains stratiform interworking architecture composite.
Example 1
8g sodium carboxymethylcelluloses are taken, 8g glucose is added in 700mL deionized waters, is stirred 20min with 300r/min, is added
200g carborundum, 50g aluminum oxide, 8g zirconium oxides, continue to be transferred in planetary high-energy ball mill after stirring 20min, with 100r/
Min ball milling 8h, obtain ceramic slurry, take Teflon mould, and control bottom temp be -30 DEG C, then by ceramic slurry with
10mL/min is sprayed into mould, after sprayed, stood directional solidification 2h, is obtained solidifying body, is placed in after solidifying body is stripped true
In vacuum freecing-dry case, 40h is freeze-dried at 1Pa, -60 DEG C, obtains layered porous ceramic body, by layered porous ceramic body
It is placed in tube furnace, 1100 DEG C is heated to 5 DEG C/min under air atmosphere, after insulation reaction 60min again under argon atmosphere,
It is heated to 1500 DEG C, room temperature is cooled to 5 DEG C/min after insulation reaction 2h, layered porous ceramics is obtained, layered porous ceramics is put
In in high-pressure impregnation stove, and the placing aluminium alloy at the top of ceramics, it is 1Pa to be evacuated to furnace pressure, then is heated to 5 DEG C/min
800 DEG C, enable aluminum alloy to melt, and it is 2MPa to be passed through argon gas to furnace pressure, is incubated after 10min and is cooled to 450 with 5 DEG C/min
DEG C, 10h is incubated, then room temperature is naturally cooled to, obtain stratiform interworking architecture composite.
Example 2
89g sodium carboxymethylcelluloses are taken, 9g glucose is added in 725mL deionized waters, is stirred 25in with 350r/min, is added
220g carborundum, 55g aluminum oxide, 9g zirconium oxides, continue to be transferred in planetary high-energy ball mill after stirring 25min, with 120r/
Min ball milling 9h, obtain ceramic slurry, take Teflon mould, and control bottom temp be -25 DEG C, then by ceramic slurry with
15mL/min is sprayed into mould, after sprayed, stood directional solidification 2h, is obtained solidifying body, is placed in after solidifying body is stripped true
In vacuum freecing-dry case, 44h is freeze-dried at 5Pa, -55 DEG C, obtains layered porous ceramic body, by layered porous ceramic body
It is placed in tube furnace, 1150 DEG C is heated to 5 DEG C/min under air atmosphere, after insulation reaction 70min again under argon atmosphere,
It is heated to 1550 DEG C, room temperature is cooled to 5 DEG C/min after insulation reaction 3h, layered porous ceramics is obtained, layered porous ceramics is put
In in high-pressure impregnation stove, and the placing aluminium alloy at the top of ceramics, it is 5Pa to be evacuated to furnace pressure, then is heated to 5 DEG C/min
850 DEG C, enable aluminum alloy to melt, and it is 2MPa to be passed through argon gas to furnace pressure, is incubated after 12min and is cooled to 470 with 5 DEG C/min
DEG C, 11h is incubated, then room temperature is naturally cooled to, obtain stratiform interworking architecture composite.
Example 3
10g sodium carboxymethylcelluloses are taken, 10g glucose is added in 750mL deionized waters, stirs 30min with 400r/min, then add
Enter 240g carborundum, 60g aluminum oxide, 10g zirconium oxides, continue to be transferred in planetary high-energy ball mill after stirring 30min, with
150r/min ball milling 10h, obtain ceramic slurry, take Teflon mould, and it is -20 DEG C to control bottom temp, then by ceramic slurry
Material is sprayed into mould with 20mL/min, after sprayed, stood directional solidification 3h, is obtained solidifying body, solidifying body is stripped rearmounted
In vacuum freezing drying oven, 48h is freeze-dried at 10Pa, -50 DEG C, obtains layered porous ceramic body, by layered porous pottery
Porcelain billet body is placed in tube furnace, and 1200 DEG C are heated to 5 DEG C/min under air atmosphere, again in argon gas after insulation reaction 80min
Under atmosphere, 1600 DEG C are heated to, room temperature is cooled to 5 DEG C/min after insulation reaction 3h, obtains layered porous ceramics, will be layered porous
Ceramics are placed in high-pressure impregnation stove, and the placing aluminium alloy at the top of ceramics, and it is 10Pa to be evacuated to furnace pressure, then with 5 DEG C/
Min is heated to 900 DEG C, enables aluminum alloy to melt, and it is 3MPa to be passed through argon gas to furnace pressure, is incubated after 15min and is dropped with 5 DEG C/min
Temperature is incubated 12h to 500 DEG C, then naturally cools to room temperature, obtains stratiform interworking architecture composite.
The extinguishing chemical that the stratiform interworking architecture composite being prepared into and Guangzhou company produce is detected, specific inspection
Survey as follows：
（1）Modulus of elasticity is tested
Modulus of elasticity is the ability for characterizing material resistance elastic deformation, is realized in this experiment by measuring ultrasonic velocity non-broken
The modulus of elasticity of material is measured under bad state.Cut out using WEDM respectively along freezing direction is parallel and perpendicular to
Size is 10 × 10 × 10mm3Cube.Pass through sonigauge（Olympus38DLPLUS, SA）Measurement ultrasonic wave exists
The longitudinal wave velocity CL and transverse wave speed CS propagated in composite different directions.Compressional wave single crystal probe（M112-RM, 10MHz）Make
By the use of glycerine as couplant, and shear wave single crystal probe（V156-RM, 5MHz）Couplant is used as using syrup.
（2）Polishing machine is tested
Dry friction and wear experiment before, friction surface, which is polished, to be treated to sample with 2000# silicon carbide papers, guarantee treat flour milling with
It is secondary to mill to completely attach to, subsequent weighed samples mass M0.Abrasion sample is positioned in acetone by frictional wear experiment after terminating, and is used
Cleaned in supersonic wave cleaning machine, the optical electrobalance for being then 0.1mg with precision weighs the mass M 1 after its wear test.With weightlessness
Method calculates the wear rate W of sample, and its calculation formula is as follows：
W=（M0-M1）/ρD
In formula, ρ is the density for wearing sample, and D is sliding distance.
（3）Fracture toughness test
Using the fracture toughness of SEN beam method (SENB) test sample.Cut using WEDM from composite
It is 2 × 4 × 20mm to cut out size3Sample, kerf width 0.25mm, notch depth 2mm, specimen surface is polished place
Reason.Three-point bending loading experiment is carried out in universal electrical Material Testing Machine (Instron5689, InstronCorp., USA),
Its span is 16mm, rate of head movement 0.05mm/min.Specific test result such as table 1.
The stratiform interworking architecture composite property of table 1 characterizes
As shown in Table 1, the obtained stratiform interworking architecture composite of the present invention, has high-modulus, high-strength tenacity, low wear rate, is
The composite lacked currently on the market, there is preferable development prospect.
Claims (6)
1. a kind of preparation method of stratiform interworking architecture composite, it is characterised in that specifically preparation process is：
（1）Row is transferred to after taking sodium carboxymethylcellulose, glucose, deionized water, carborundum, aluminum oxide, zirconium oxide well mixed
8 ~ 10h of ball milling, obtains ceramic slurry in planetary high energy ball mill；
（2）Ceramic slurry is sprayed into Teflon mould, 2 ~ 3h of directional solidification is stood, obtains solidifying body；
（3）40 ~ 48h of freeze-drying in vacuum freezing drying oven is placed in after solidifying body is stripped, obtains layered porous ceramic body；
（4）Layered porous ceramic body is placed in tube furnace and sintered, is cooled to room temperature, obtains layered porous ceramics；
（5）Layered porous ceramics are placed in high-pressure impregnation stove, and the placing aluminium alloy at the top of ceramics, vacuumize and be heated to
800 ~ 900 DEG C are enabled aluminum alloy to melt, and 450 ~ 500 DEG C of 10 ~ 12h of insulation are cooled to after being passed through 10 ~ 15min of argon pressurization, then natural
Room temperature is cooled to, obtains stratiform interworking architecture composite.
A kind of 2. preparation method of stratiform interworking architecture composite as claimed in claim 1, it is characterised in that step（1）
The parts by weight of each component raw material are：8 ~ 10 parts of sodium carboxymethylcelluloses, 8 ~ 10 parts of glucose, 700 ~ 750 parts of deionized waters,
200 ~ 240 parts of carborundum, 50 ~ 60 parts of aluminum oxide, 8 ~ 10 parts of zirconium oxides.
A kind of 3. preparation method of stratiform interworking architecture composite as claimed in claim 1, it is characterised in that step（2）
The directional solidification is to control Teflon mould bottom temp as -30 ~ -20 DEG C, then by ceramic slurry with 10 ~ 20mL/min
It is sprayed into mould.
A kind of 4. preparation method of stratiform interworking architecture composite as claimed in claim 1, it is characterised in that step（3）
Pressure is 1 ~ 10Pa in the vacuum freezing drying oven, and temperature is -60 ~ -50 DEG C.
A kind of 5. preparation method of stratiform interworking architecture composite as claimed in claim 1, it is characterised in that step（4）
The sintering process is to be warming up to 1100 ~ 1200 DEG C, 60 ~ 80min of insulation reaction under air atmosphere with 5 DEG C/min, then in argon
Atmosphere is warming up to 1500 ~ 1600 DEG C, 2 ~ 3h of insulation reaction under enclosing, the heating, cooling speed is 5 DEG C/min.
A kind of 6. preparation method of stratiform interworking architecture composite as claimed in claim 1, it is characterised in that step（5）
The high-pressure impregnation furnace pressure is 1 ~ 10Pa, and the moulding pressure is 2 ~ 3MPa.
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| CN108994301B (en) * | 2018-07-03 | 2021-03-26 | 中国科学院金属研究所 | Metal-based bionic composite material reinforced by nano carbon material and preparation method thereof |
| CN109180195A (en) * | 2018-09-30 | 2019-01-11 | 威海威林特电控科技有限公司 | One kind is based on adding obdurability porous ceramic composite and its preparation process made of infiltrated metal method |
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| CN112851316A (en) * | 2021-01-21 | 2021-05-28 | 清远市简一陶瓷有限公司 | Light-transmitting brick and preparation method thereof |
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